#------------------------------------------------------------------------------ #$Date: 2019-10-11 03:39:08 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219264 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234527.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7234527 loop_ _publ_author_name 'Nayak, Biswajit' 'Halder, Senjuti' 'De, Sagnik' 'Das, Gopal' _publ_section_title ; Binding Consistency of Anion by Effect of Aromatic Meta-Substitution of Bis-urea Receptors: Entrapment of Hexafluorosilicate Clusters ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C9CE01485C _journal_year 2019 _chemical_formula_moiety '2(C22 H16 N6 O2), 2(C16 H36 N), F6 Si' _chemical_formula_sum 'C76 H104 F6 N14 O4 Si' _chemical_formula_weight 1419.82 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-09-13 deposited with the CCDC. 2019-10-10 downloaded from the CCDC. ; _cell_angle_alpha 89.154(6) _cell_angle_beta 79.572(5) _cell_angle_gamma 87.827(5) _cell_formula_units_Z 1 _cell_length_a 11.6125(7) _cell_length_b 12.4000(9) _cell_length_c 13.7567(10) _cell_measurement_reflns_used 2521 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.3930 _cell_measurement_theta_min 3.6060 _cell_volume 1946.7(2) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies,Version 1.171.37.35' _computing_data_collection 'CrysAlisPro, Agilent Technologies,Version 1.171.37.35' _computing_data_reduction 'CrysAlisPro, Agilent Technologies,Version 1.171.37.35 ' _computing_molecular_graphics 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_publication_material 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'ccd area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_unetI/netI 0.0681 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 13769 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.049 _diffrn_reflns_theta_max 25.048 _diffrn_reflns_theta_min 2.993 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.211 _exptl_crystal_description needle _exptl_crystal_F_000 758 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.101 _exptl_transmission_factor_max 0.990 _exptl_transmission_factor_min 0.974 _refine_diff_density_max 0.718 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.052 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 461 _refine_ls_number_reflns 6878 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.166 _refine_ls_R_factor_all 0.1422 _refine_ls_R_factor_gt 0.0857 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2315 _refine_ls_wR_factor_ref 0.2754 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3673 _reflns_number_total 6878 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce01485c2.cif _cod_data_source_block L1-SiF6 _cod_database_code 7234527 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; exp_3578.res created by SHELXL-2014/7 TITL CF solution in P-1 CELL 0.71073 11.61251 12.4 13.75675 89.1537 79.572 87.8274 ZERR 1 0.00066 0.00087 0.00099 0.0058 0.0054 0.0051 LATT 1 SFAC C H N O F Si UNIT 76 104 14 4 6 1 OMIT -3 50.1 L.S. 20 ACTA BOND FMAP 2 PLAN 10 DFIX 1.54 0.02 C26 C25 WGHT 0.100000 1.000000 FVAR 5.72069 SI1 6 0.000000 1.000000 0.000000 10.50000 0.06386 0.04693 = 0.04129 -0.00060 -0.01028 0.01116 F2 5 0.132650 0.954169 0.014833 11.00000 0.08048 0.09708 = 0.08490 0.01099 -0.01790 0.01622 F1 5 -0.033536 1.031270 0.118573 11.00000 0.12027 0.08965 = 0.05452 -0.00886 -0.01073 0.01221 F3 5 -0.048051 0.875860 0.025787 11.00000 0.09322 0.06161 = 0.10101 -0.00204 0.00431 0.00667 O1 4 0.811926 0.421428 1.136746 11.00000 0.10112 0.06421 = 0.05210 -0.01328 -0.01706 0.03143 O2 4 0.705713 0.193958 0.727418 11.00000 0.08561 0.05899 = 0.07325 -0.00988 -0.03580 0.00967 N3 3 0.889153 0.309742 1.009487 11.00000 0.07695 0.05380 = 0.04529 -0.01428 -0.01881 0.01712 AFIX 43 H3N 2 0.926490 0.249425 0.993966 11.00000 -1.20000 AFIX 0 N2 3 0.897852 0.258948 1.168422 11.00000 0.08256 0.05049 = 0.04230 -0.01051 -0.01638 0.01535 AFIX 43 H2N 2 0.937399 0.203562 1.141768 11.00000 -1.20000 AFIX 0 N4 3 0.792327 0.218214 0.860944 11.00000 0.10046 0.05089 = 0.04196 -0.00391 -0.02167 -0.00357 AFIX 43 H4N 2 0.807633 0.184407 0.912404 11.00000 -1.20000 AFIX 0 N5 3 0.773996 0.048847 0.805513 11.00000 0.10251 0.05003 = 0.05699 0.00215 -0.03536 -0.00201 AFIX 43 H5N 2 0.795446 0.029483 0.860015 11.00000 -1.20000 AFIX 0 C9 1 0.858472 0.375737 0.932471 11.00000 0.05929 0.05454 = 0.04192 -0.00538 -0.01073 0.00711 C14 1 0.809928 0.329827 0.857412 11.00000 0.06760 0.05165 = 0.04127 -0.00717 -0.01165 0.00318 C15 1 0.753747 0.157005 0.792248 11.00000 0.06557 0.05353 = 0.04720 -0.00537 -0.00867 0.00305 C8 1 0.862513 0.336907 1.107275 11.00000 0.06110 0.05476 = 0.05253 -0.01177 -0.01747 0.00890 C7 1 0.873053 0.264385 1.272565 11.00000 0.06487 0.06197 = 0.04451 -0.00734 -0.01256 0.00929 N7 3 0.352086 0.272058 0.803415 11.00000 0.06885 0.06930 = 0.07859 -0.00556 0.00633 0.01216 C16 1 0.763380 -0.033889 0.739321 11.00000 0.06136 0.04918 = 0.05900 -0.00123 -0.01248 -0.00807 C18 1 0.690107 -0.113673 0.606451 11.00000 0.06836 0.05589 = 0.06285 -0.01322 -0.01626 0.00262 C17 1 0.693272 -0.026414 0.667577 11.00000 0.07197 0.05533 = 0.06084 -0.01176 -0.01676 0.00893 AFIX 43 H17 2 0.648990 0.036372 0.660633 11.00000 -1.20000 AFIX 0 C6 1 0.870320 0.360503 1.322362 11.00000 0.08179 0.06673 = 0.04698 -0.01204 -0.01932 0.01668 AFIX 43 H6 2 0.886240 0.424802 1.287732 11.00000 -1.20000 AFIX 0 C13 1 0.782848 0.395936 0.781572 11.00000 0.09266 0.05758 = 0.05281 -0.00027 -0.02653 -0.00578 AFIX 43 H13 2 0.750677 0.366310 0.731268 11.00000 -1.20000 AFIX 0 C10 1 0.876741 0.486067 0.930133 11.00000 0.07344 0.06253 = 0.06353 -0.01026 -0.02482 -0.00238 AFIX 43 H10 2 0.908831 0.516499 0.980105 11.00000 -1.20000 AFIX 0 C20 1 0.755907 -0.207983 0.614517 11.00000 0.08309 0.05281 = 0.08397 -0.01513 -0.01812 -0.00087 AFIX 43 H20 2 0.752453 -0.266068 0.573267 11.00000 -1.20000 AFIX 0 C1 1 0.853831 0.169090 1.324945 11.00000 0.12238 0.06683 = 0.05587 0.00262 -0.01707 0.00059 AFIX 43 H1 2 0.858232 0.103806 1.291823 11.00000 -1.20000 AFIX 0 C31 1 0.225205 0.278401 0.790171 11.00000 0.05327 0.09491 = 0.11638 0.00105 0.00522 0.01173 AFIX 23 H31A 2 0.179002 0.241187 0.845509 11.00000 -1.20000 H31B 2 0.198876 0.353653 0.793729 11.00000 -1.20000 AFIX 0 C37 1 0.408780 -0.030787 0.875302 11.00000 0.19749 0.06827 = 0.15809 -0.00355 0.05265 -0.02196 AFIX 23 H37A 2 0.492555 -0.021053 0.866129 11.00000 -1.20000 H37B 2 0.384461 -0.071131 0.936030 11.00000 -1.20000 AFIX 0 C32 1 0.199052 0.233232 0.697666 11.00000 0.06789 0.17579 = 0.14805 -0.04133 -0.02269 0.01813 AFIX 23 H32A 2 0.237802 0.162686 0.686283 11.00000 -1.20000 H32B 2 0.229794 0.279719 0.642467 11.00000 -1.20000 AFIX 0 C33 1 0.071137 0.223232 0.702536 11.00000 0.07807 0.30861 = 0.16128 -0.00374 -0.02026 0.03021 AFIX 23 H33A 2 0.038786 0.191837 0.766166 11.00000 -1.20000 H33B 2 0.036138 0.295299 0.700289 11.00000 -1.20000 AFIX 0 C34 1 0.035641 0.160796 0.627493 11.00000 0.08556 0.31352 = 0.14972 0.01224 -0.02354 -0.01664 AFIX 137 H34A 2 0.052201 0.198608 0.565419 11.00000 -1.50000 H34B 2 -0.046911 0.149397 0.644361 11.00000 -1.50000 H34C 2 0.077758 0.092384 0.622223 11.00000 -1.50000 AFIX 0 C22 1 0.828518 -0.128821 0.746289 11.00000 0.08046 0.05609 = 0.08481 -0.00022 -0.03515 -0.00119 AFIX 43 H22 2 0.875360 -0.135099 0.794367 11.00000 -1.20000 AFIX 0 C19 1 0.619371 -0.109897 0.530316 11.00000 0.10721 0.07405 = 0.08709 -0.03312 -0.04136 0.02586 C4 1 0.843424 0.359852 1.425058 11.00000 0.09499 0.07457 = 0.05188 -0.01540 -0.02080 0.02433 C27 1 0.431193 0.330752 0.720995 11.00000 0.06341 0.07156 = 0.06464 -0.00414 0.00232 0.00613 AFIX 23 H27A 2 0.427981 0.295599 0.659066 11.00000 -1.20000 H27B 2 0.511128 0.322458 0.732294 11.00000 -1.20000 AFIX 0 C11 1 0.848189 0.551391 0.855079 11.00000 0.09430 0.05332 = 0.06559 0.00443 -0.02257 -0.00532 AFIX 43 H11 2 0.859088 0.625311 0.854991 11.00000 -1.20000 AFIX 0 C3 1 0.820292 0.265552 1.477897 11.00000 0.16264 0.09243 = 0.04375 -0.00025 -0.00910 0.02287 AFIX 43 H3 2 0.799968 0.266404 1.546457 11.00000 -1.20000 AFIX 0 C12 1 0.802995 0.504391 0.780001 11.00000 0.10338 0.06322 = 0.05730 0.00928 -0.02821 -0.00173 AFIX 43 H12 2 0.786057 0.546916 0.727781 11.00000 -1.20000 AFIX 0 N6 3 0.565940 -0.111852 0.468857 11.00000 0.17153 0.11250 = 0.11343 -0.05447 -0.07482 0.05043 C23 1 0.355174 0.319547 0.903287 11.00000 0.09920 0.09069 = 0.06572 -0.00046 0.01447 0.02036 AFIX 23 H23A 2 0.303408 0.279257 0.952897 11.00000 -1.20000 H23B 2 0.323717 0.393180 0.903978 11.00000 -1.20000 AFIX 0 N1 3 0.827273 0.541034 1.516993 11.00000 0.26305 0.10238 = 0.09168 -0.05459 -0.04256 0.05306 C28 1 0.402661 0.450652 0.709531 11.00000 0.10052 0.07486 = 0.09199 0.00429 0.01412 0.01079 AFIX 23 H28A 2 0.330483 0.459399 0.683660 11.00000 -1.20000 H28B 2 0.390140 0.484246 0.774001 11.00000 -1.20000 AFIX 0 C21 1 0.825626 -0.213675 0.684095 11.00000 0.08463 0.04686 = 0.10532 0.00016 -0.02967 0.00910 AFIX 43 H21 2 0.871735 -0.275675 0.689521 11.00000 -1.20000 AFIX 0 C35 1 0.399321 0.155582 0.798429 11.00000 0.07032 0.06815 = 0.10082 0.00214 0.00396 0.00833 AFIX 23 H35A 2 0.392157 0.126550 0.734790 11.00000 -1.20000 H35B 2 0.482151 0.155513 0.801381 11.00000 -1.20000 AFIX 0 C24 1 0.474050 0.320699 0.933289 11.00000 0.11339 0.12881 = 0.07045 -0.02257 -0.00379 0.01266 AFIX 23 H24A 2 0.520782 0.376636 0.897390 11.00000 -1.20000 H24B 2 0.515512 0.251670 0.919519 11.00000 -1.20000 AFIX 0 C5 1 0.835218 0.461134 1.477648 11.00000 0.15114 0.09549 = 0.05965 -0.02645 -0.03289 0.04072 C2 1 0.827782 0.171312 1.427788 11.00000 0.17622 0.08979 = 0.05662 0.01768 -0.01653 0.00439 AFIX 43 H2 2 0.815253 0.106863 1.462881 11.00000 -1.20000 AFIX 0 C29 1 0.496237 0.505745 0.643291 11.00000 0.11739 0.09500 = 0.10250 0.02144 -0.01297 -0.00617 AFIX 23 H29A 2 0.511037 0.468853 0.580329 11.00000 -1.20000 H29B 2 0.567221 0.498467 0.671061 11.00000 -1.20000 AFIX 0 C30 1 0.472843 0.622993 0.624518 11.00000 0.15381 0.09079 = 0.13780 0.02074 -0.02752 -0.03216 AFIX 137 H30A 2 0.412860 0.630818 0.584943 11.00000 -1.50000 H30B 2 0.543280 0.654313 0.590203 11.00000 -1.50000 H30C 2 0.447380 0.659077 0.686362 11.00000 -1.50000 AFIX 0 C25 1 0.450720 0.343574 1.046539 11.00000 0.12832 0.22318 = 0.17110 -0.10398 -0.05791 0.06349 AFIX 23 H25A 2 0.406894 0.411409 1.060671 11.00000 -1.20000 H25B 2 0.406553 0.286277 1.082769 11.00000 -1.20000 AFIX 0 C26 1 0.561278 0.348335 1.072803 11.00000 0.28501 0.17603 = 0.13579 -0.05260 -0.00584 -0.00620 AFIX 137 H26A 2 0.606395 0.283573 1.052054 11.00000 -1.50000 H26B 2 0.552501 0.355101 1.143211 11.00000 -1.50000 H26C 2 0.600813 0.409598 1.041168 11.00000 -1.50000 AFIX 0 C36 1 0.340464 0.080822 0.878228 11.00000 0.11857 0.08445 = 0.18551 0.03339 0.05532 0.01880 AFIX 23 H36A 2 0.260822 0.069931 0.869154 11.00000 -1.20000 H36B 2 0.337038 0.113558 0.942341 11.00000 -1.20000 AFIX 0 C38 1 0.380062 -0.083556 0.795460 11.00000 0.18515 0.14676 = 0.27282 0.01891 -0.07756 0.00410 AFIX 137 H38A 2 0.297994 -0.097810 0.808446 11.00000 -1.50000 H38B 2 0.424736 -0.150457 0.785181 11.00000 -1.50000 H38C 2 0.397538 -0.038996 0.737382 11.00000 -1.50000 AFIX 0 HKLF 4 REM CF solution in P-1 REM R1 = 0.0857 for 3673 Fo > 4sig(Fo) and 0.1422 for all 6878 data REM 461 parameters refined using 1 restraints END WGHT 0.1019 2.0708 REM Highest difference peak 0.718, deepest hole -0.346, 1-sigma level 0.052 Q1 1 0.4163 0.2840 1.1321 11.00000 0.05 0.72 Q2 1 0.0906 0.2639 0.6330 11.00000 0.05 0.33 Q3 1 0.5029 -0.0590 0.8840 11.00000 0.05 0.28 Q4 1 0.0685 1.0613 0.0598 11.00000 0.05 0.27 Q5 1 0.4750 -0.0500 0.9420 11.00000 0.05 0.22 Q6 1 0.0206 0.9263 0.0778 11.00000 0.05 0.21 Q7 1 0.4975 0.4781 0.7736 11.00000 0.05 0.21 Q8 1 0.5896 0.4714 0.6044 11.00000 0.05 0.20 Q9 1 0.8721 0.1830 1.1568 11.00000 0.05 0.20 Q10 1 0.3268 -0.1405 0.8949 11.00000 0.05 0.19 ; _shelx_res_checksum 39899 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Si1 Si 0.0000 1.0000 0.0000 0.0509(5) Uani 1 2 d S . P F2 F 0.1327(2) 0.9542(3) 0.0148(2) 0.0877(9) Uani 1 1 d . . . F1 F -0.0335(3) 1.0313(3) 0.1186(2) 0.0891(9) Uani 1 1 d . . . F3 F -0.0481(3) 0.8759(2) 0.0258(2) 0.0882(9) Uani 1 1 d . . . O1 O 0.8119(3) 0.4214(3) 1.1367(2) 0.0728(10) Uani 1 1 d . . . O2 O 0.7057(3) 0.1940(3) 0.7274(2) 0.0702(9) Uani 1 1 d . . . N3 N 0.8892(3) 0.3097(3) 1.0095(2) 0.0581(10) Uani 1 1 d . . . H3N H 0.9265 0.2494 0.9940 0.070 Uiso 1 1 calc R U . N2 N 0.8979(3) 0.2589(3) 1.1684(2) 0.0582(10) Uani 1 1 d . . . H2N H 0.9374 0.2036 1.1418 0.070 Uiso 1 1 calc R U . N4 N 0.7923(3) 0.2182(3) 0.8609(3) 0.0633(10) Uani 1 1 d . . . H4N H 0.8076 0.1844 0.9124 0.076 Uiso 1 1 calc R U . N5 N 0.7740(4) 0.0488(3) 0.8055(3) 0.0673(11) Uani 1 1 d . . . H5N H 0.7954 0.0295 0.8600 0.081 Uiso 1 1 calc R U . C9 C 0.8585(4) 0.3757(4) 0.9325(3) 0.0519(10) Uani 1 1 d . . . C14 C 0.8099(4) 0.3298(3) 0.8574(3) 0.0534(11) Uani 1 1 d . . . C15 C 0.7537(4) 0.1570(4) 0.7922(3) 0.0557(11) Uani 1 1 d . . . C8 C 0.8625(4) 0.3369(4) 1.1073(3) 0.0554(11) Uani 1 1 d . . . C7 C 0.8731(4) 0.2644(4) 1.2726(3) 0.0570(11) Uani 1 1 d . . . N7 N 0.3521(3) 0.2721(3) 0.8034(3) 0.0750(12) Uani 1 1 d . . . C16 C 0.7634(4) -0.0339(4) 0.7393(3) 0.0562(11) Uani 1 1 d . . . C18 C 0.6901(4) -0.1137(4) 0.6065(3) 0.0618(12) Uani 1 1 d . . . C17 C 0.6933(4) -0.0264(4) 0.6676(3) 0.0623(12) Uani 1 1 d . . . H17 H 0.6490 0.0364 0.6606 0.075 Uiso 1 1 calc R U . C6 C 0.8703(4) 0.3605(4) 1.3224(3) 0.0646(13) Uani 1 1 d . . . H6 H 0.8862 0.4248 1.2877 0.078 Uiso 1 1 calc R U . C13 C 0.7828(4) 0.3959(4) 0.7816(3) 0.0659(13) Uani 1 1 d . . . H13 H 0.7507 0.3663 0.7313 0.079 Uiso 1 1 calc R U . C10 C 0.8767(4) 0.4861(4) 0.9301(3) 0.0649(12) Uani 1 1 d . . . H10 H 0.9088 0.5165 0.9801 0.078 Uiso 1 1 calc R U . C20 C 0.7559(4) -0.2080(4) 0.6145(4) 0.0728(14) Uani 1 1 d . . . H20 H 0.7525 -0.2661 0.5733 0.087 Uiso 1 1 calc R U . C1 C 0.8538(5) 0.1691(4) 1.3249(4) 0.0817(16) Uani 1 1 d . . . H1 H 0.8582 0.1038 1.2918 0.098 Uiso 1 1 calc R U . C31 C 0.2252(4) 0.2784(5) 0.7902(5) 0.0911(18) Uani 1 1 d . . . H31A H 0.1790 0.2412 0.8455 0.109 Uiso 1 1 calc R U . H31B H 0.1989 0.3537 0.7937 0.109 Uiso 1 1 calc R U . C37 C 0.4088(9) -0.0308(6) 0.8753(7) 0.151(4) Uani 1 1 d . . . H37A H 0.4926 -0.0211 0.8661 0.182 Uiso 1 1 calc R U . H37B H 0.3845 -0.0711 0.9360 0.182 Uiso 1 1 calc R U . C32 C 0.1991(5) 0.2332(7) 0.6977(6) 0.130(3) Uani 1 1 d . . . H32A H 0.2378 0.1627 0.6863 0.156 Uiso 1 1 calc R U . H32B H 0.2298 0.2797 0.6425 0.156 Uiso 1 1 calc R U . C33 C 0.0711(7) 0.2232(10) 0.7025(8) 0.184(5) Uani 1 1 d . . . H33A H 0.0388 0.1918 0.7662 0.221 Uiso 1 1 calc R U . H33B H 0.0361 0.2953 0.7003 0.221 Uiso 1 1 calc R U . C34 C 0.0356(7) 0.1608(10) 0.6275(7) 0.183(5) Uani 1 1 d . . . H34A H 0.0522 0.1986 0.5654 0.274 Uiso 1 1 calc R U . H34B H -0.0469 0.1494 0.6444 0.274 Uiso 1 1 calc R U . H34C H 0.0778 0.0924 0.6222 0.274 Uiso 1 1 calc R U . C22 C 0.8285(4) -0.1288(4) 0.7463(4) 0.0713(14) Uani 1 1 d . . . H22 H 0.8754 -0.1351 0.7944 0.086 Uiso 1 1 calc R U . C19 C 0.6194(5) -0.1099(5) 0.5303(4) 0.0869(17) Uani 1 1 d . . . C4 C 0.8434(5) 0.3599(4) 1.4251(4) 0.0734(15) Uani 1 1 d . . . C27 C 0.4312(4) 0.3308(4) 0.7210(4) 0.0685(13) Uani 1 1 d . . . H27A H 0.4280 0.2956 0.6591 0.082 Uiso 1 1 calc R U . H27B H 0.5111 0.3225 0.7323 0.082 Uiso 1 1 calc R U . C11 C 0.8482(4) 0.5514(4) 0.8551(4) 0.0700(13) Uani 1 1 d . . . H11 H 0.8591 0.6253 0.8550 0.084 Uiso 1 1 calc R U . C3 C 0.8203(6) 0.2656(5) 1.4779(4) 0.102(2) Uani 1 1 d . . . H3 H 0.8000 0.2664 1.5465 0.122 Uiso 1 1 calc R U . C12 C 0.8030(5) 0.5044(4) 0.7800(4) 0.0731(14) Uani 1 1 d . . . H12 H 0.7861 0.5469 0.7278 0.088 Uiso 1 1 calc R U . N6 N 0.5659(6) -0.1119(5) 0.4689(4) 0.127(2) Uani 1 1 d . . . C23 C 0.3552(5) 0.3195(5) 0.9033(4) 0.0895(18) Uani 1 1 d . . . H23A H 0.3034 0.2793 0.9529 0.107 Uiso 1 1 calc R U . H23B H 0.3237 0.3932 0.9040 0.107 Uiso 1 1 calc R U . N1 N 0.8273(7) 0.5410(5) 1.5170(4) 0.152(3) Uani 1 1 d . . . C28 C 0.4027(5) 0.4507(4) 0.7095(4) 0.0935(18) Uani 1 1 d . . . H28A H 0.3305 0.4594 0.6837 0.112 Uiso 1 1 calc R U . H28B H 0.3901 0.4842 0.7740 0.112 Uiso 1 1 calc R U . C21 C 0.8256(5) -0.2137(4) 0.6841(4) 0.0777(15) Uani 1 1 d . . . H21 H 0.8717 -0.2757 0.6895 0.093 Uiso 1 1 calc R U . C35 C 0.3993(4) 0.1556(4) 0.7984(4) 0.0825(16) Uani 1 1 d . . . H35A H 0.3922 0.1265 0.7348 0.099 Uiso 1 1 calc R U . H35B H 0.4822 0.1555 0.8014 0.099 Uiso 1 1 calc R U . C24 C 0.4740(6) 0.3207(6) 0.9333(4) 0.106(2) Uani 1 1 d . . . H24A H 0.5208 0.3766 0.8974 0.127 Uiso 1 1 calc R U . H24B H 0.5155 0.2517 0.9195 0.127 Uiso 1 1 calc R U . C5 C 0.8352(6) 0.4611(5) 1.4776(4) 0.101(2) Uani 1 1 d . . . C2 C 0.8278(6) 0.1713(5) 1.4278(4) 0.109(2) Uani 1 1 d . . . H2 H 0.8153 0.1069 1.4629 0.130 Uiso 1 1 calc R U . C29 C 0.4962(6) 0.5057(5) 0.6433(5) 0.106(2) Uani 1 1 d . . . H29A H 0.5110 0.4689 0.5803 0.127 Uiso 1 1 calc R U . H29B H 0.5672 0.4985 0.6711 0.127 Uiso 1 1 calc R U . C30 C 0.4728(7) 0.6230(5) 0.6245(6) 0.127(3) Uani 1 1 d . . . H30A H 0.4129 0.6308 0.5849 0.190 Uiso 1 1 calc R U . H30B H 0.5433 0.6543 0.5902 0.190 Uiso 1 1 calc R U . H30C H 0.4474 0.6591 0.6864 0.190 Uiso 1 1 calc R U . C25 C 0.4507(8) 0.3436(9) 1.0465(7) 0.171(5) Uani 1 1 d D . . H25A H 0.4069 0.4114 1.0607 0.205 Uiso 1 1 calc R U . H25B H 0.4066 0.2863 1.0828 0.205 Uiso 1 1 calc R U . C26 C 0.5613(11) 0.3483(9) 1.0728(7) 0.202(5) Uani 1 1 d D . . H26A H 0.6064 0.2836 1.0521 0.304 Uiso 1 1 calc R U . H26B H 0.5525 0.3551 1.1432 0.304 Uiso 1 1 calc R U . H26C H 0.6008 0.4096 1.0412 0.304 Uiso 1 1 calc R U . C36 C 0.3405(6) 0.0808(5) 0.8782(6) 0.141(3) Uani 1 1 d . . . H36A H 0.2608 0.0699 0.8692 0.169 Uiso 1 1 calc R U . H36B H 0.3370 0.1136 0.9423 0.169 Uiso 1 1 calc R U . C38 C 0.3801(10) -0.0836(9) 0.7955(10) 0.198(5) Uani 1 1 d . . . H38A H 0.2980 -0.0978 0.8084 0.296 Uiso 1 1 calc R U . H38B H 0.4247 -0.1505 0.7852 0.296 Uiso 1 1 calc R U . H38C H 0.3975 -0.0390 0.7374 0.296 Uiso 1 1 calc R U . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0639(10) 0.0469(10) 0.0413(9) -0.0006(7) -0.0103(7) 0.0112(8) F2 0.0805(19) 0.097(2) 0.085(2) 0.0110(17) -0.0179(15) 0.0162(16) F1 0.120(2) 0.090(2) 0.0545(17) -0.0089(15) -0.0107(15) 0.0122(18) F3 0.093(2) 0.0616(18) 0.101(2) -0.0020(16) 0.0043(17) 0.0067(15) O1 0.101(2) 0.064(2) 0.0521(19) -0.0133(15) -0.0171(16) 0.0314(19) O2 0.086(2) 0.059(2) 0.073(2) -0.0099(16) -0.0358(18) 0.0097(17) N3 0.077(2) 0.054(2) 0.045(2) -0.0143(17) -0.0188(17) 0.0171(19) N2 0.083(3) 0.050(2) 0.042(2) -0.0105(16) -0.0164(17) 0.0154(19) N4 0.100(3) 0.051(2) 0.042(2) -0.0039(17) -0.0217(19) -0.004(2) N5 0.103(3) 0.050(2) 0.057(2) 0.0021(18) -0.035(2) -0.002(2) C9 0.059(3) 0.055(3) 0.042(2) -0.0054(19) -0.0107(19) 0.007(2) C14 0.068(3) 0.052(3) 0.041(2) -0.0072(19) -0.012(2) 0.003(2) C15 0.066(3) 0.054(3) 0.047(3) -0.005(2) -0.009(2) 0.003(2) C8 0.061(3) 0.055(3) 0.053(3) -0.012(2) -0.017(2) 0.009(2) C7 0.065(3) 0.062(3) 0.045(2) -0.007(2) -0.013(2) 0.009(2) N7 0.069(3) 0.069(3) 0.079(3) -0.006(2) 0.006(2) 0.012(2) C16 0.061(3) 0.049(3) 0.059(3) -0.001(2) -0.012(2) -0.008(2) C18 0.068(3) 0.056(3) 0.063(3) -0.013(2) -0.016(2) 0.003(2) C17 0.072(3) 0.055(3) 0.061(3) -0.012(2) -0.017(2) 0.009(2) C6 0.082(3) 0.067(3) 0.047(3) -0.012(2) -0.019(2) 0.017(3) C13 0.093(3) 0.058(3) 0.053(3) 0.000(2) -0.027(2) -0.006(3) C10 0.073(3) 0.063(3) 0.064(3) -0.010(2) -0.025(2) -0.002(2) C20 0.083(3) 0.053(3) 0.084(4) -0.015(3) -0.018(3) -0.001(3) C1 0.122(5) 0.067(3) 0.056(3) 0.003(3) -0.017(3) 0.001(3) C31 0.053(3) 0.095(4) 0.116(5) 0.001(4) 0.005(3) 0.012(3) C37 0.197(9) 0.068(5) 0.158(8) -0.004(5) 0.053(7) -0.022(5) C32 0.068(4) 0.176(8) 0.148(7) -0.041(6) -0.023(4) 0.018(4) C33 0.078(5) 0.309(15) 0.161(9) -0.004(9) -0.020(5) 0.030(7) C34 0.086(5) 0.314(15) 0.150(9) 0.012(9) -0.024(5) -0.017(7) C22 0.080(3) 0.056(3) 0.085(4) 0.000(3) -0.035(3) -0.001(3) C19 0.107(4) 0.074(4) 0.087(4) -0.033(3) -0.041(3) 0.026(3) C4 0.095(4) 0.075(4) 0.052(3) -0.015(3) -0.021(3) 0.024(3) C27 0.063(3) 0.072(3) 0.065(3) -0.004(2) 0.002(2) 0.006(2) C11 0.094(4) 0.053(3) 0.066(3) 0.004(2) -0.023(3) -0.005(3) C3 0.163(6) 0.092(5) 0.044(3) 0.000(3) -0.009(3) 0.023(4) C12 0.103(4) 0.063(3) 0.057(3) 0.009(2) -0.028(3) -0.002(3) N6 0.172(5) 0.112(5) 0.113(4) -0.054(4) -0.075(4) 0.050(4) C23 0.099(4) 0.091(4) 0.066(4) 0.000(3) 0.014(3) 0.020(3) N1 0.263(8) 0.102(5) 0.092(4) -0.055(4) -0.043(5) 0.053(5) C28 0.101(4) 0.075(4) 0.092(4) 0.004(3) 0.014(3) 0.011(3) C21 0.085(4) 0.047(3) 0.105(4) 0.000(3) -0.030(3) 0.009(3) C35 0.070(3) 0.068(3) 0.101(4) 0.002(3) 0.004(3) 0.008(3) C24 0.113(5) 0.129(6) 0.070(4) -0.023(4) -0.004(3) 0.013(4) C5 0.151(6) 0.095(5) 0.060(3) -0.026(3) -0.033(3) 0.041(4) C2 0.176(7) 0.090(5) 0.057(4) 0.018(3) -0.017(4) 0.004(4) C29 0.117(5) 0.095(5) 0.103(5) 0.021(4) -0.013(4) -0.006(4) C30 0.154(7) 0.091(5) 0.138(6) 0.021(4) -0.028(5) -0.032(5) C25 0.128(7) 0.223(11) 0.171(9) -0.104(8) -0.058(6) 0.063(7) C26 0.285(15) 0.176(11) 0.136(8) -0.053(7) -0.006(9) -0.006(10) C36 0.119(5) 0.084(5) 0.186(8) 0.033(5) 0.055(5) 0.019(4) C38 0.185(10) 0.147(10) 0.273(15) 0.019(9) -0.078(10) 0.004(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 F1 Si1 F1 180.0 . 2_575 F1 Si1 F2 89.41(15) . 2_575 F1 Si1 F2 90.59(15) 2_575 2_575 F1 Si1 F2 90.59(15) . . F1 Si1 F2 89.41(15) 2_575 . F2 Si1 F2 180.0 2_575 . F1 Si1 F3 89.77(15) . 2_575 F1 Si1 F3 90.23(15) 2_575 2_575 F2 Si1 F3 88.34(15) 2_575 2_575 F2 Si1 F3 91.66(15) . 2_575 F1 Si1 F3 90.23(15) . . F1 Si1 F3 89.77(15) 2_575 . F2 Si1 F3 91.66(15) 2_575 . F2 Si1 F3 88.34(15) . . F3 Si1 F3 180.0 2_575 . C8 N3 C9 123.5(3) . . C8 N2 C7 123.8(3) . . C15 N4 C14 127.7(4) . . C15 N5 C16 126.8(4) . . C10 C9 C14 119.4(4) . . C10 C9 N3 120.7(4) . . C14 C9 N3 119.9(4) . . C13 C14 C9 118.8(4) . . C13 C14 N4 122.6(4) . . C9 C14 N4 118.6(4) . . O2 C15 N4 124.0(4) . . O2 C15 N5 123.5(4) . . N4 C15 N5 112.6(4) . . O1 C8 N3 123.3(4) . . O1 C8 N2 123.7(4) . . N3 C8 N2 113.0(4) . . C1 C7 C6 119.9(4) . . C1 C7 N2 117.9(4) . . C6 C7 N2 122.3(4) . . C23 N7 C31 106.7(4) . . C23 N7 C27 111.7(4) . . C31 N7 C27 111.9(4) . . C23 N7 C35 110.6(4) . . C31 N7 C35 110.9(4) . . C27 N7 C35 105.2(3) . . C22 C16 C17 118.3(4) . . C22 C16 N5 117.2(4) . . C17 C16 N5 124.5(4) . . C17 C18 C20 121.7(4) . . C17 C18 C19 121.4(4) . . C20 C18 C19 116.9(4) . . C18 C17 C16 119.2(4) . . C7 C6 C4 119.1(5) . . C12 C13 C14 120.8(4) . . C11 C10 C9 121.4(4) . . C21 C20 C18 118.5(5) . . C7 C1 C2 119.5(5) . . C32 C31 N7 116.8(4) . . C38 C37 C36 104.7(10) . . C31 C32 C33 111.5(7) . . C34 C33 C32 116.9(8) . . C21 C22 C16 121.7(4) . . N6 C19 C18 176.6(6) . . C3 C4 C6 121.5(5) . . C3 C4 C5 119.1(5) . . C6 C4 C5 119.3(5) . . N7 C27 C28 116.0(4) . . C10 C11 C12 118.6(5) . . C2 C3 C4 118.6(5) . . C13 C12 C11 121.0(4) . . N7 C23 C24 116.2(4) . . C29 C28 C27 112.4(5) . . C20 C21 C22 120.6(4) . . C36 C35 N7 115.8(4) . . C23 C24 C25 106.2(5) . . N1 C5 C4 178.3(7) . . C3 C2 C1 121.4(6) . . C28 C29 C30 115.8(6) . . C26 C25 C24 105.7(8) . . C35 C36 C37 111.0(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Si1 F1 1.655(3) . Si1 F1 1.655(3) 2_575 Si1 F2 1.668(3) 2_575 Si1 F2 1.668(3) . Si1 F3 1.669(3) 2_575 Si1 F3 1.669(3) . O1 C8 1.220(5) . O2 C15 1.210(5) . N3 C8 1.369(5) . N3 C9 1.417(5) . N2 C8 1.372(5) . N2 C7 1.411(5) . N4 C15 1.368(5) . N4 C14 1.406(5) . N5 C15 1.368(5) . N5 C16 1.405(5) . C9 C10 1.391(6) . C9 C14 1.400(6) . C14 C13 1.390(6) . C7 C1 1.379(7) . C7 C6 1.380(6) . N7 C23 1.510(7) . N7 C31 1.516(6) . N7 C27 1.519(6) . N7 C35 1.523(6) . C16 C22 1.387(6) . C16 C17 1.389(6) . C18 C17 1.386(6) . C18 C20 1.387(6) . C18 C19 1.443(7) . C6 C4 1.391(6) . C13 C12 1.373(7) . C10 C11 1.382(6) . C20 C21 1.360(7) . C1 C2 1.393(7) . C31 C32 1.483(8) . C37 C38 1.384(12) . C37 C36 1.566(9) . C32 C33 1.485(10) . C33 C34 1.427(12) . C22 C21 1.371(7) . C19 N6 1.137(7) . C4 C3 1.377(8) . C4 C5 1.450(8) . C27 C28 1.523(7) . C11 C12 1.385(7) . C3 C2 1.357(8) . C23 C24 1.511(8) . N1 C5 1.129(7) . C28 C29 1.469(8) . C35 C36 1.509(8) . C24 C25 1.561(10) . C29 C30 1.496(8) . C25 C26 1.399(11) .